Process plant sample collection system and method

ABSTRACT

This disclosure sets out a method and apparatus for extracting repeated process samples. Each sample is put into a segregated bottle or container and the container is dated and time stamped. The containers are arranged in sequence on a feed system and are filled in sequence and marked.

BACKGROUND OF THE DISCLOSURE

Consider the testing of a chemical processing plant which is placed online and operates indefinitely. Periodically, it is necessary to testthe product made in the plant. That is a difficult task to accomplish inmany circumstances, especially those where the process operates at veryhigh pressures and temperatures. Typically, high pressures andtemperatures making it difficult to obtain a sample. Moreover, expensivemetals and expensive fabrication techniques are required to enable theprocessing plant to be properly confined within the structure whichholds the process. This remains a problem even when only a small sampleis required for periodic testing. Not only must the sample be removedfrom the process plant, the sample must be delivered into a samplecontainer for easy transportation to a lab for testing. Consider as anexample a petrochemical processing plant where a process is carried outat elevated temperatures of over 1000° F. and very high pressureslimited primarily by the pressure rating of the equipment of the samplecollection system. The fluid flowing in the process pipes and pressurevessels of the processing plant may flow at a rate of hundreds ofgallons per minute, and yet only a small portion is required fortesting, for example, one liter.

There is even the possibility that the sample will change from a gas toliquid on reducing the temperature and pressure while removing thesample. Transfer of the sample from the interior of a process plantthrough the walls of the pipes or other pressure vessels which containthe process requires tapping the process to obtain the sample, and thismust be done without permitting the sample to escape to atmosphere.Except in rare cases, such a sample is at least partially, and oftenextremely volatile. In any event, a sample must be removed from theprocessing plant, transferred through a set of flow lines, metered intosome sort of sample container, and then delivered for subsequenttesting, for instance, at a testing laboratory sample analysis or othertesting can be carried out. One mode of testing is to fill a smallsample container, carry it to the testing lab, and conduct the testthere. This enables a single testing lab to test samples from severaldifferent locations on a process plant. For instance, a single processplant may comprise several different columns with intermediate stages ofprocessing, thereby generating samples at 10 or 20 different locations;samples are obtained at different times of the day from the severalsample locations, the tests are then run, and product quality and purityis then certified as a result of the laboratory testing.

The present apparatus and method enable periodic testing to be carriedout in this fashion. This disclosure sets forth a means and mechanismfor such testing notwithstanding the fact that testing is required ofthe product when the product is manufactured at extremely high pressuresand temperatures. There is a problem in transfer of the sample. Forinstance, as a result of high process temperatures, the removed producttypically will be a gas, and will tend to be reduced in size should itundergo a phase of conversion from gas to liquid. On the other hand,because of extremely high pressures, a sample will tend to expand whenthe pressure confinement is reduced. It is therefore somewhat difficultto scale the amount of sample to be removed so that the proper size andconsistent size of sample can be provided in a sample container. Thepresent apparatus enables this to be accomplished. Moreover, it isaccomplished in the context where one or several sample containers areserially filled with each separated from the other at the sample takingdevice. The timed separation of samples is accomplished by providingfixed flow lines extending to the sample receiving container which areperiodically purged with nitrogen to assure that there is no remnant ofsample gas in the lines for later sample collection. The purging oflines assures that two samples taken hours apart are not mixed seriallyby storage in the connective lines. Moreover, this is all accomplishedwithout permitting fugitive emissions to atmosphere. In part, that isprevented and protected against by utilization of a closed housing whichis maintained under a blanket of nitrogen. This assures that there willbe minimal accumulation of explosive gases in the housing, or gaseswhich otherwise create some type of hazard. Finally, the system operatesso that it can be cyclically controlled by a handle for the purpose ofperiodic operation of a two position, six port valve. In another form,operation is by a motor and timer. A sample taking system may beoperated periodically to obtain or remove a sample from a system. Oneaspect of the present invention is the provision of a small samplemeasuring loop connected to a six port valve. A small loop is a storagecontainer. It is however relatively small. It stores a specifiedquantity of the sample. One suitable quantity of sample is one cubiccentimeter. This is normally written as one cc. It is possible toconnect a sample storage loop of this limited capacity to a six port,two way valve. That is, the sample storage loop serves a meter device toassure that the sample is sized to the size required. In addition tothat, the present disclosure sets forth a sample container system whichcan be adapted for receipt of a measured small sample. Assume forpurposes of discussion that a sample is required once per hour. By usinga larger container, twenty-four samples taken in a single day can bestored in the container. They are mixed or blended. That may forsufficient to laboratory testing to provide an assay later. On the otherhand, the sample may require uniquely separate treating and testing. Forexample, this can occur in the instance that a small sample is taken andthe small sample is put into a container and not mixed with any othersample. In that instance, the sample container should be sized to thesame size or one cubic centimeter.

The present disclosure sets forth a system which provides such a samplemechanism. The sample mechanism in this instance is provided with aprocession of single sample containers which are scaled so that thevolume of the container matches the volume in the sample loop. In theexample just mentioned, one cc of samples obtained and stored in acontainer which has a capacity of one cc. Perhaps, there will be amodest amount of head room in the sample container beneath the coveredmouth and septum over the mouth of the container. In that instance, onesample can be taken per hour and twenty four different containers willbe filled. Each of the several containers is filled in the describedmanner. Each container is provided with this measured amount.

The measured volume introduced into the container is received into thecontainer and stored so that spillage or commingling is avoided. In theexample given, to obtain one sample per hour, twenty four separatecontainers are required. The present disclosure provides an indexingmechanism which aligns a series of containers for syringe filling. Eachis filled individually. A mechanism is further disclosed which labelseach of the containers. Typically, the containers look alike and bearsimilar markings on exterior. They are filled with the same fluidalthough the fluid may differ from moment to moment as a result tochanges in the operating process. For sample taking purposes and to havean acceptable assay of the separate samples, it is necessary to labelthe individual containers. That is done in the present disclosure by alabel printing mechanism. To the extent that the system operates withseveral different containers, each is labeled so that they can beindividually tested at a remote laboratory either in sequence or in anymixed sequence. The results are nevertheless readily able to be isolatedto a particular time of day. This may tell much about the operation ofthe plan. In one example, the plant may be susceptible to sun load. Atthe night the plant operating characteristics might change because thesun load is reduced. This could produce a different product purity,perhaps differing only slightly, but perhaps differing substantially. Itis possible for the product to be sufficiently out of the requiredspecifications for that product stream that the product is momentarilysubstandard. The product can be produced in such a fashion to beexceedingly rich, and thereby unduly expensive. That is just as great aproblem as being substandard.

In summary, the present disclosure is a system for transfer of a sampleby means of permanently made connections to a process across a flowrestriction in the process. Connection is through an inlet line andoutlet line. These connections extend to two ports on a six port valve.There is a sample storage loop in the six port valve. The sample storageloop includes a sized volumetric buffer tank or sample line. It is sizedso that the sample that is delivered at the prevailing pressure andtemperature is held in this buffer tank. To the extent that there iseither expansion or contraction by transfer out of the process plant toa reduced pressure and a temperature approaching ambient, there issufficient size in the buffer tank to permit a properly sized sample tobe collected. The tank can be large or small. A purge gas sourceconnected to a needle valve with a flow meter connects to a fifth port,and the sixth valve port is connected by means of a sample lineextending to a syringe needle for filling a closed sample container. Asequence of operations is also set forth where the sample is deliveredfor intermediate holding and later for delivery into the samplereceiving container. In addition to that, the equipment operates in asequence to direct a continuous flow of nitrogen for purging of theconnective lines. The sample from the system can be collected in a largecontainer holding several samples (e.g., samples from one day ofoperation) or can be stored in a small container sized to store onesmall sample. In this instance, sample containers are marked as they areserially sequentially filled.

BRIEF DESCRIPTION OF THE DRAWINGS

So that the manner in which the above recited features, advantages andobjects of the present invention are attained and can be understood indetail, more particular description of the invention, briefly summarizedabove, may be had by reference to the embodiments thereof which areillustrated in the appended drawings.

It is to be noted, however, that the appended drawings illustrate onlytypical embodiments of this invention and are therefore not to beconsidered limiting of its scope, for the invention may admit to otherequally effective embodiments.

FIG. 1 is a schematic of the sample collecting apparatus of the presentdisclosure showing a system where the material to be sampled flowsthrough the circulate pathway and is returned by the process and thebuffer tank is empty while a nitrogen purge occurs;

FIG. 2 of the drawings shows the system of FIG. 1 after switching sothat connections are altered for filling the buffer tank which is asequential step in comparison with the arrangement shown in FIG. 1 ofthe drawings;

FIGS. 3-6 sequentially show different steps involved in filling a samplecontainer including the steps of purging the storage loop and samplecontainer in FIG. 3, filling the sample loop in FIG. 4 while continuingto purge, emptying the sample loop with purge gas to fill the samplecontainer, and then blocking flow so the sample container can beremoved, the sample loop purged, and discharging any surplus of thespecimen through the filter;

FIG. 7 is a side view of a magazine loading mechanism which delivers anumber of individual sample holding containers serially along a troughwhich positions the sample containers beneath a pair of syringes forfilling wherein individual sample containers are filled and subsequentlynumbered with a suitable code number and dumped into a storagecontainer; and

FIG. 8 is a plan view of the trough shown in FIG. 7 further showingdetails of a detent mechanism so that only one sample container issupplied for each operation.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT

In the drawings, the numeral 10 identifies the sample collectionapparatus of the present disclosure. This apparatus is constructedwithin a cabinet 12 which comprises a closed housing. Preferably, it ismade of sheet metal, but in many instances, it can be an explosion proofhousing or cabinet. To increase and enhance the safety of the system itmay be helpful dependent on the type of material being sampled to fillthis housing with a blanket of nitrogen. A nitrogen source 14 provides aflow of nitrogen through a feed which in turn connects with a needlevalve 16, the needle valve being input to the housing 12 to fill theinterior with nitrogen. It is desirable to do this in instances wherethe material being tested tends to form an explosive mixture with air,or perhaps poses some other threat. The remainder of the equipment ispreferably located in the housing 12. Conveniently, the housing 12 canbe provided with an optional door. The door 18 permits operator handlingof the sample receiving container 20 which is installed for holding of ameasured sample. Typically, the container 20 is sized to a particularsize such as one liter. Typically, it is a closed vessel which iscovered over with a cap at the narrow neck or throat of the container.The cap has a hold provided in it large enough to receive the samplingneedles and captures a rubber/Teflon laminated sheet of materialfunctioning as a septum. The septum is a healing membrane which ispunctured but does not leak.

Operation of the system will be described in detail after reviewing theapparatus involved in the present disclosure. To this end, there is avalve 22 which is connected with some aspect of a manufacturing processsuch as in a distillation column, cat cracker and the like. The valve 22is spaced from a similar valve 24. They are located so that there issome small pressure drop between the two. This enables the inlet line 26to receive a flow of the process fluid. The inlet line 26 is similar tothe outlet line 28 which returns surplus fluid to the process. In atypical circumstance, the pressure in the lines 26 and 28 issubstantially the same, and can be easily as high as 500 psi but thereis a differential of about 5 or 10 psi. Higher pressures can be handledby heavy duty equipment.

A filter 30 is serially connected in the inlet valve 26. In turn, thenline 26 also connects with a two position, six port valve 32. The valvehas a valve body with a rotor on the interior which is rotated typicallyby 60° at the urging of a motor 34 connected to the rotor. The motor isperiodically operated by a timer 36 to rotate by 60°. This changes thealignment of the ports as will be observed in contrasting FIG. 1 andFIG. 2 of the drawings. Hand operation of the valve is also possible.

The system has other connections to the valve 32. The numeral 40identifies a line which loops from one port to another report on thevalve 32 and serially connects with a buffer tank 42. The tank 42 is anintermediate location which holds the desired quantity of sample. Morewill be noted regarding the purpose of this intermediate holding step,and especially the amount held at that location.

The nitrogen supply 14 connects through an adjustable needle valve 46which serially introduces nitrogen flow through a flow meter 48. Theflow meter 48 is preferably mounted so that it can be viewed. Thisassures the operator that nitrogen gas is flowing into the system forpurging of the lines as will be described. Another connection to thevalve is provided by the sample line 50 which is terminated at a syringeneedle 52. That needle introduces sample into the storage container 20.The storage container 20 also provides an outlet for gas in the bottle20 which is removed through a similar syringe needle 54, flowing in aline 56, and then, in the form of waste products, is delivered through afilter system 60 and vented to atmosphere. The filter 60 is packed witha material which absorbs and purifies the discharge so that thedischarged atmosphere is substantially inert, meaning primarily nitrogengas flow through an atmospheric discharge passage 62. If desired, theoutlet 62 can be connected with a flare in the event that the materialcan be combusted readily.

DETAILED DESCRIPTION OF THE METHOD OF FILLING AND PURGING

Attention is now directed to FIG. 2 of the drawings for a description ofa filling and purging sequence. This description will particularly focuson those things which occur when the raw sample is being obtained fromthe process plant In FIG. 2 of the drawings, the valve 32 is positionedso that there is a flow path in the following sequence, namely processfluid is delivered through the inlet line 26, flowing into a line 64,the buffer tank 42, the line 40 and back through the valve 32 and to theoutlet line 28. As an example, assume that this position of theequipment is maintained for a few minutes so that the process fluidcirculates several times through this route. After this, time assuresthat all the lines and especially the buffer tank 42 are filled with theprocess fluid, and that is accomplished without dilution. Recalling thatthe process fluid may be at several hundred psi pressure, and elevatedtemperature, there is a connection of any needed short or long distanceto the present system. Whatever the case, and assuming a requisiteinterval for circulation in the connected lines just described, thevalve 32 is operated from the position shown in FIG. 2 to the positionshown in FIG. 1. The position in FIG. 1 will be described as the fillingposition. Filling focuses primarily on filling the container 42. In thefilling position shown in FIG. 2, there is sufficient pressuredifferential to cause continued flow along the path described. There mayhowever be a phase change dependent on the cooling interval afterswitching the valve 32 from the position shown in FIG. 2 of the drawingsto the postiion shown in FIG. 1. This movement positions the valve sothat there is a completley different arrangement of the connectionsthrough the valve and that will be described as the sampling position.The sampling position occurs in the following fashion. The timer 36 inconjunction with the motor 34 moves the valve by 60°. This breaks theconnection which was accomplished in the loop 40, and completelyreconnects the loop 40. This new flow sequence will then be describedbeginning with the nitrogen source 14. Nitrogen is delivered ratablythrough the needle valve 46, through the flow regulator 48, and the line66. The nitrogen flows through the valve 32 and into the sample loop 40into the buffer tank 42. Fluid continues to flow through the line 64back through the valve 32, the line 50 and the syringe 52 for fillingthe sample receiving container 20. In brief, the nitrogen is deliveredat a flow rate and for an interval sufficient to force the atmospherethat was initially in the container 20 out of the container. Thecontainer 20 is voided through the filter 60. Moreover, this nitrogenflow path continues to operate so that a sufficient quantity of thesample is forced from the buffer tank 42 along the flow path into theremovable sample receiving container 20 to file it to a desirable level.Vapors contained within the container 20 are forced out through thefilter but that does not pose a problem with fugitive emissions as aresult of the filter operation.

Operator attendance is involved in the present apparatus by removal of afilled sample container 20 and replacement of it with an empty samplecontainer. If a sample is taken every day, then the container 20 isremoved daily and replaced. Removal requires pulling the samplecontainer 20 downwardly so that the two syringe needles retract from theseptum. This seals the interior. A new sample container is installed byremoval of the metal cap over the septum, and pushing the container 20upwardly so that the two needles are inserted through the septum forfilling. This periodic removal and replacement assures that individualsamples can be taken at the requisite interval, removed from the areaand taken to a test lab, and yet the equipment is left in a condition sothat another sample can be collected.

FIGS. 3-6

Jointly, FIGS. 3-6 show a sequence of operations using the device ofFIG. 1. In this instance, it has been enhanced by the incorporation of ablocking valve 66 which functions in a manner to be described. Tounderstand the sequence of operation, the valve 32 has been operated sothat process fluid circulates but is not sampled. Rather, the purged gas(normally nitrogen in most instances) is delivered in the ordinaryfashion, and flows through the valve 32 because the blocking valve 66 isopened. This flow of purge gas is delivered to the sample storage loop40. This includes the tank 42. However, an alternate size can be usedincluding sizes sufficiently larger if the sample is one liter orbigger, or is so small that the sample is only about one cc, or evensmaller if desired. In any case, this part of the system is purged bydelivery of the purge gas to clear the lines to assure that the processequipment lines do not bias the test data from remnants of a prior testleft in the system.

FIG. 4 of the drawings shows the valve 32 operated by rotation through60°. In this instance, the sample loop 40 is connected with the processand the sample loop is filled. The sample loop 40 is permitted to befilled during continuous circulation for an adequate time interval toassure that the loop 40 is filled with essentially pure sample material.While this is occurring in that part of the equipment, the purge gasflow is directed through the blocking valve 66 and is then deliveredinto the sample container 20 and flows from the sample container 20through the filter 60. This purges the lines which interconnect from thepurge gas source through the sample container.

The next involves operation of the valve 32. This is shown in FIG. 5 ofthe drawings. After it is operated to the position shown the valve 32 isrestored to the position shown in FIG. 3 of the drawings. The sample isthen isolated in the sample loop 40. Recall again that this loop has alarge or small capacity as required. The sample loop is then cleared bydelivery of the purge gas through the blocking valve 66, the samplestorage loop 40 and into the sample container 20. Delivery is continuedfor a sufficient interval to assure that the flow clears all the sampleinto the container. Any surplus is directed through the filter 60 alongwith the purge gas. Here, it is especially helpful to note that thesample storage loop can be changed in size. It can be as large or smallas needed. It can be large or small to match the container 20. Moreover,the container 20 is filled to the desired level of the container. If thecontainer is as large as one liter, it is readily handled. If thecontainer is as small as one cc, it is small and is handled in adifferent fashion. Additional apparatus regarding the handling of thesmall containers will be disclosed and described. In any case, FIG. 5shows the sequence of operations in which the sample is transferred fromthe sized sample loop 40 into the sample container 20.

FIG. 6 of the drawings shows the last position of the equipment. At thispoint in time, the blocking valve 66 is closed to prevent the flow ofnitrogen. The sample loop 40 has been cleared. The lines connecting withthe filter 60 have also been cleared by the purge gas. The samplecontainer 20 can then be removed from the syringe needles and a newbottle placed on the syringe needles. The process is also isolated atthis moment. This enables a sample container to be placed on the syringeneedles so that the equipment is restored to the operative state shownin FIG. 3. The sequence of steps is repeated beginning with thearrangement shown in FIG. 3 then to FIG. 4, filling which isaccomplished in FIG. 5 and sample container removal which is then shownin FIG. 6.

FIGS. 7 AND 8 CONSIDERED JOINTLY

Attention is now directed to FIGS. 7 and 8 which show a mechanism forhandling a number of duplicate sample containers. In this aspect,attention is first directed to the side view of the equipment whichhandles a plurality of duplicate containers. An elongate trough 70supports a series of containers which are delivered from a containersource. They traverse the trough 70. They are typically arranged so thatthe containers to stand erect. This enables the top end of all thecontainers be aligned for filling through the syringe needles. Thecontainers are forced along the pathway defined by the trough 70. Asshown in the plan view, a set of detents 72 is used to hold the lastcontainer supported by the trough. That container is forced out of thetrough in a controlled fashion. In one aspect of this, the containers inthe trough are pushed by a ram 74 at the left hand end of the trough inFIG. 8. When the trough is filled with sample containers, the stroke ofthe ram 74 is readily controlled. Moreover, a reciprocating ram 74 ispreferably used wherein a connective rod 76 extends to the ram andprovides reciprocating motion to the ram 74 from a double actinghydraulic or pneumatic cylinder 78. This indexes the containers 20 bythe width of one container. The containers are held against accidentalmisregistration. The detents assure that the containers are fed singly.

Returning now to FIG. 7 of the drawings, this structure further includesa mechanism for transporting a single container. The mechanismincorporates a circular platform with a semi-circular skirt which isidentified at 80. This is positioned adjacent to the end of the troughso that a single container is forced into a cradled position. It issupported beneath and on the for side. Since movement is from left toright, this assists in seating each individual container. When seated,the container is held so that it can then be forced upwardly against thesyringe needles thereabove. The needles 52 and 54 are again shown inthis view. They are part of the system 10 shown in FIG. 1 of thedrawings. When this occurs, the cradled container is held in theuppermost position stabbed by the two syringes, and the fillingoperation can then occur. This requires movement of the container 20between three positions. The first position occurs after the containerhas been delivered from the trough 70 and is cradled by the means 80. Ahydraulic cylinder 82 is used to extend a piston rod upwardly to movethe container to the installed position or the second position in thissequence of operations. After the container has been filled, thecontainer can then be moved downwardly to a third position. Thatrequires retraction of the extending piston rod 84. When retracted, itmoves the individual container to an aligned location for marking. Thelocation for marking positions the container 20 so that a symbol can beprinted on it. This involves the operation of a time and date clock.This forms a suitable signal which is then input to an ink jet printer.Once the hydraulic cylinder has retracted to the third position, thecontainer that had just been filled is positioned immediately oppositethe ink jet printer. A suitable symbol is printed on the side of thecontainer. As an example, the container can be marked with a bar codesymbol, or other indicia of time and date. It can be directly readableor can be provided in a code form.

The time and date clock 86 provides a suitable instruction signal to theink jet printer 88 which enables it to form the unique containersmarkings. When that occurs, then the container can be dumped. In oneaspect of the present disclosure, a motor 90 is mechanically connectedto the cylinder 82 to impart rotation. The cylinder is rotated so thatthe container cradled on the device is then dumped. It can be dumpedinto a large basket or other receptacle (not shown) for the containers20. If this receptacle is filled in one day, and samples are taken everyhour, twenty four uniquely marked containers are received in thereceptacle. Even over a long weekend, as many as 48 or 72 containers canbe appropriately received and stored. This is especially helpful forequipment which runs around the clock throughout most of the year. Thisenables the production to be measured and assayed for testing in alaboratory. Again, the performance of the system can be measured andknown periodically.

In one aspect, the apparatus shown in FIGS. 7 and 8 is a system whichprovides multiple containers of some suitable size. Actually, thecontainers can be as large or small as needed. Typically, a one litercontainer is relatively large while a container for one cc is relativelysmall in diameter and typically is not very tall. It will typicallymeasure from about 2 to about 4 cm in height. If it is unduly small, theink jet printer 88 can print on a label which is adhesively glued to orotherwise attached to the individual container. In any event, theindividual containers are tagged or labeled with a suitable code symbolto enable the sample in the container to be uniquely associated with theproduction flow at a particular time and on a particular day. For thatreason, the system is able to provide a regular indication of time anddate. This especially helps in the isolation of individual samples in alarge sample lot which is periodically taken to a test laboratory.

The apparatus of FIG. 7 can be used with the structure shown in FIG. 1.In that particular instance, it may be necessary to align the samplecontainer 20 and the transport mechanism as shown in FIG. 7 so that thesample container is properly aligned with the syringe needles 52 and 54.

The motor 34 and the timer 36 are preferably powered electrically withlow voltage to reduce explosion risk. In some instances, they can be gaspowered, for instance, by the purge gas flow. In that case, the risk ofspark initiated explosion is further reduced. Likewise, the cylindersand motors in FIGS. 7 and 8 can be pneumatic powered.

While the foregoing is directed to the preferred embodiments, the scopeis determined by the claims which follow.

I claim:
 1. A method of collecting a plurality of samples from a process operating at a process pressure, comprising the steps of:(a) connecting a sample input line to said process and flowing a sized sample from said process through said sample input line and through a valve means and into a sized sample measuring means comprising a sized buffer tank; (b) filling said sized sample to a selected ambient pressure within said sized buffer tank, wherein said ambient pressure is lower than said process pressure; (c) delivering said sized sample from said sized buffer tank through said valve means and through a sample delivery means and into a sized sample container in a plurality of sized sample containers; (d) clocking and controlling the accurance of sized sample delivery with a clock, and marking said sized sample container with said clocked accurance and removing said sized sample container containing said sized sample from said sample delivery means; (e) forming a time dependent indicator based upon said clocking for said sized sample container so that said sized sample is uniquely identified to distinguish said sample: (f) purging said sized buffer tank and said valve means and said sample delivery means with purge gas after said sample delivery; (g) positioning another sized sample container from said plurality of sized sample containers to receive another sized sample from said sample delivery means; and (h) repeating steps (b) through (g).
 2. The method of claim 1 wherein:(a) said plurality of said sized sample containers is aligned serially along a guide surface pathway; (b) positioning said pathway cooperatively to enable each of said sample receiving container to move sequentially into operative connection with respect to said sample delivery means; (c) delivering the sized sample from said sample delivery means responsive to a gas drive for delivery of said sized sample to said sized sample container; and (d) wherein said time of said sized sample delivery of each said sized sample container is measured and controlled by said clock.
 3. The method of claim 2 wherein said gas drive is supplied to said sized buffer tank through said valve means to initiate said delivery of said sized sample to said sized sample container.
 4. The method of claim 3 wherein said valve means is a multiport valve with multiple settings, and said sized buffer tank is hydraulically isolated from said process when said valve is set in a first position.
 5. The method of claim 3 wherein said valve means is a multiport valve with multiple settings, and said sized buffer tank is hydraulically connected to said process to fill said sized buffer tank with said sized sample when said valve is set in a second position.
 6. The method of claim 3 wherein said valve means is a multiport valve with multiple settings, and said sized buffer tank is hydraulically connected to said gas drive and said sized sample container when said valve is set in a third position, and said sized sample is delivered from said sized buffer tank and through said valve and into said sized sample container by said gas drive.
 7. The method of claim 4 wherein said sized buffer tank and said valve means and said sample delivery means are purged with said purge gas from said gas drive when said valve is set in said first position.
 8. The method of claim 1 wherein:(a) said sample delivery means comprises a pair of syringe needles; (b) said sized sample container comprises a septum; and (c) said pair of syringe needles punctures said septum and said sized sample is delivered to said sized sample container through a first needle of said pair of said syringe needles.
 9. The method of claim 8 wherein said purge gas is flowed through said valve means and through said first syringe needle, and waste products are flowed from said sized sample container and into a filter container through a second needle of said pair of syringe needles.
 10. The method of claim 3 wherein said valve means is a multiport valve with multiple settings, and said valve moves between said multiple settings as determined by a motor.
 11. The method of claim 1 wherein said sized sample container is sized to receive and store a single said sized sample.
 12. The method of claim 11 wherein each of said plurality of sized sample containers is filled with said single sized sample in timed sequence by a means moving each of said sized sample containers into operative connection with respect to said sample delivery means. 